CN104550984A - Preparation method of nickel-based high-temperature alloy powder for 3D (Three Dimensional) printing - Google Patents
Preparation method of nickel-based high-temperature alloy powder for 3D (Three Dimensional) printing Download PDFInfo
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- CN104550984A CN104550984A CN201410779257.1A CN201410779257A CN104550984A CN 104550984 A CN104550984 A CN 104550984A CN 201410779257 A CN201410779257 A CN 201410779257A CN 104550984 A CN104550984 A CN 104550984A
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Abstract
The invention discloses a preparation method of nickel-based high-temperature alloy powder for 3D (Three Dimensional) printing. According to the method, high-performance nickel-based high-temperature alloy powder, which meets the requirement of 3D printing, is obtained through vacuum smelting, degassing, refining, atomization and sieving technologies of nickel-based high-temperature alloy. The problem of difficulty in preparation of the low-cost high-performance nickel-based high-temperature alloy powder for the 3D printing process is solved. The method has the characteristics of simplicity, effectiveness and low cost, the oxygen content of the gas atomized nickel-based high-temperature alloy powder can be obviously reduced, and the sphericity and the fine powder yield of the powder are improved.
Description
Technical field
The present invention is a kind of preparation method of 3D printing Ni-base Superalloy Powder, belongs to powder metallurgical technology.
Background technology
3D prints (increasing material manufacture), and technology has become one of emerging technology paid close attention to most in the whole world at present, and its proprietary material especially Aero-Space high-performance high-temperature nickel-base alloy component 3D printing powder prospect of industrial development is fine.
High-performance high-temperature nickel-base alloy component 3D printing technique is started in early 1990s, technology difficulty is larger, the high-power energy beam of main employing is if laser or electron beam are as thermal source, dusty material is made to carry out selective melting, formed strictly by the accumulation horizon manufactured and designed after crystallisation by cooling, accumulation horizon is continuously shaped, forms final products.Up to the present, industrial micro metal component 3D prints relatively easy, and the 3D of the hardware that volume is larger prints difficulty very greatly, and the requirement controlled materials and process is very high.This, by being the emphasis direction that 3D prints the development of Industrial driving related industries, also will be a key technology.Its maximum difficulty is material and moulding process.
High-performance high-temperature nickel-base alloy component 3D printing technique is from coming out beginning, just inseparable with the development of supplementary material.In recent years, nickel base superalloy component directly manufactures used high-performance high-temperature nickel-base alloy dusty material and receives much concern.The 3D of following nickel base superalloy, titanium alloy material band large-scale metal component prints and does to become the research direction of major technique.But the domestic main dependence on import of material printed for hardware 3D, and price is high, and external high-quality 3D printing Ni-base Superalloy Powder price is everlasting 800 yuan/more than kg.The domestic research that there is no for being exclusively used in the powder preparation that 3D prints, some unit adopts conventional gas-atomised powders to substitute and uses, there is a lot of unworthiness, the problems such as such as oxygen content is high, sphericity is poor, size distribution is not good, this limits the high-end 3D of China to a certain extent and prints further developing of industry.Print field at high-performance metal component 3D, China is in the urgent need to Ni-based, the cobalt-based Ni-base Superalloy Powder of low oxygen content, fine grain, high sphericity, and powder size is below 50 microns, and oxygen content should lower than 0.02%, and good sphericity.
But, Ni-base Superalloy Powder atomization process is extremely complicated, relate to hydrodynamics, materialogy, physical chemistry etc. multidisciplinary, by material physical property, melting characteristic parameter, parameters of the guiding vane with atomization parameter various factors coupling is interactional affects, only have various factors coupling optimal design, just can prepare high-quality spherical low-oxygen Ni-base Superalloy Powder.
Summary of the invention
The present invention designs for above-mentioned prior art situation the preparation method providing a kind of 3D printing Ni-base Superalloy Powder just, its objective is with low cost prepare particle diameter less than 50 μm, oxygen content lower than 0.015% high sphericity Ni-base Superalloy Powder, meet the needs that 3D prints technique, promote that 3D prints the raising of quality of item.
The object of the invention is to be achieved through the following technical solutions:
The preparation method of this kind of 3D printing Ni-base Superalloy Powder, is characterized in that: the step of this preparation method is:
Step one: vacuum melting:
Nickel base superalloy foundry alloy bar is loaded in the crucible of powder by atomization stove, under lower than the vacuum of 0.1Pa, adopt intermediate frequency power supply eddy-current heating bar;
Step 2: degassed: after foundry alloy fusing, vacuum outgas 15min ~ 20min;
Step 3: refining: be filled with high-purity argon gas to 0.1MPa in powder by atomization stove, by the foundry alloy liquation of melting at 1600 DEG C ~ 1650 DEG C temperature range inside holding 10min ~ 15min;
Step 4: atomization: the foundry alloy liquation of melting is flowed down through mozzle with the mass flowrate of 5kg/min ~ 10kg/min, with the high pressure of 3MPa ~ 5MPa, high-purity argon gas, metal liquid stream is broken into fine drop, drop is through supercooling and solidify formation spherical powder, enters and receives in powder tank;
Step 5: screening: powder is after fully cooling, and sieve under high-purity argon gas atmosphere, Sieving and casing less than 50 μm powder carry out Vacuum Package;
Described high-purity argon gas purity is 99.999wt%, and wherein oxygen content is less than 0.0001wt%.
Technical solution of the present invention is in research process, powder by atomization through the analog study of hydrodynamics method machine and tens of heat is tested, disclose the formation mechenism of spherical low-oxygen Ni-base Superalloy Powder, grasp the multifactor affecting laws to Ni-base Superalloy Powder quality such as material physical property, melting characteristic parameter, parameters of the guiding vane and atomization parameter, explore the process of preparing of applicable 3D printing Ni-base Superalloy Powder.
Technical solution of the present invention processes in each technological process all to adopt an effective measure prevent the increase of oxygen content in power in vacuum melting, degassed, refining, atomization, screening, guarantees the requirement that final Ni-base Superalloy Powder oxygen content reaches 3D and prints.Vacuum required in technical scheme is less than 0.1Pa, inflation and atomization and uses the oxygen content of high-purity argon gas lower than 0.0001wt%, and should to sieve under high-purity argon gas atmosphere, is all the oxidation in order to avoid Ni-base Superalloy Powder.3D printing technique requires high to Ni-base Superalloy Powder sphericity in addition, good fluidity, the density of such powder are high, low quality of molten metal flow rate is adopted in the technical program, to improve gas liquid ratio, increase the cooling velocity of molten drop, obtain the Ni-base Superalloy Powder that sphericity is higher, the oxygen content of powder is below 0.015%, and the powder yield of powder diameter less than 50 μm is more than 90%, significantly reduces powder cost.
The advantage of technical solution of the present invention is: Ni-base Superalloy Powder has comparatively low oxygen content, high sphericity, and recovery rate is higher, powder diameter less than 50 μm Ni-base Superalloy Powder recovery rates are more than 90%, cost is lower, make final Ni-base Superalloy Powder meet the high standard of 3D printing technique, meet the requirement that 3D prints technique.
Accompanying drawing explanation
Fig. 1 is the size distribution curve of case study on implementation 1 gained In718 alloy powder
Fig. 2 is the pattern photo of case study on implementation 1 gained In718 alloy powder
Fig. 3 is the size distribution curve of case study on implementation 2 gained FGH96 alloy powder
Fig. 4 is the pattern photo of case study on implementation 2 gained FGH96 alloy powder
Detailed description of the invention
Below with reference to drawings and Examples, technical solution of the present invention is further described:
Embodiment 1:
The step that employing technical solution of the present invention prepares 3D printing Ni-base Superalloy Powder method is as follows:
(1) vacuum melting: 150kgIn718 nickel base superalloy foundry alloy bar is thrown in the crucible of powder by atomization stove, adopt intermediate frequency power supply eddy-current heating bar under 0.08Pa vacuum;
(2) degassed: after foundry alloy fusing, vacuum outgas 15min;
(3) refining: be filled with high-purity argon gas to 0.1MPa in stove, high-purity argon gas purity is 99.999wt%, in argon gas, oxygen content is 0.00005%, by the molten metal of melting at 1600 DEG C of insulation 15min;
(4) be atomized: flowed down through mozzle with the weight flow rate of 5kg/min by molten metal, be broken into fine drop by the high pressure of 3MPa, high-purity argon gas, drop is through supercooling and solidify formation spherical powder, enter and receive in powder tank;
(5) sieve: powder is after fully cooling, and sieve under high-purity argon gas atmosphere, Sieving and casing less than 50 μm powder carry out Vacuum Package.
By analysis, prepared nickel base superalloy In718 oxygen content in power is 0.0094%-0.012%, can be found out by Fig. 1,2, and particle diameter less than 50 μm powder yields reach 95%, and powder sphericity is better.
Embodiment 2:
The step that employing technical solution of the present invention prepares 3D printing Ni-base Superalloy Powder method is as follows:
(1) vacuum melting: 200kgFGH96 nickel base superalloy foundry alloy bar is thrown in the crucible of powder by atomization stove, adopt intermediate frequency power supply eddy-current heating bar under 0.05Pa vacuum;
(2) degassed: after foundry alloy fusing, vacuum outgas 20min;
(3) refining: be filled with high-purity argon gas to 0.1MPa in stove, high-purity argon gas purity is 99.999wt%, in argon gas, oxygen content is 0.00006wt%, by the molten metal of melting at 1640 DEG C of insulation 15min;
(4) be atomized: flowed down through mozzle with the weight flow rate of 8kg/min by molten metal, metal liquid stream is broken into fine drop by high pressure, the high-purity argon gas of employing 4MPa, and drop is through supercooling and solidify formation spherical powder, enters and receives in powder tank;
(5) sieve: powder is after fully cooling, and sieve under high-purity argon gas atmosphere, Sieving and casing less than 50 μm powder carry out Vacuum Package.
By analysis, prepared FGH96 Ni-base Superalloy Powder oxygen content is 0.0093%, can be found out by Fig. 3,4, and particle diameter less than 50 μm powder yields reach 91%, and powder sphericity is better.
Claims (1)
1. a preparation method for 3D printing Ni-base Superalloy Powder, is characterized in that: the step of this preparation method is:
Step one: vacuum melting:
Nickel base superalloy foundry alloy bar is loaded in the crucible of powder by atomization stove, under lower than the vacuum of 0.1Pa, adopt intermediate frequency power supply eddy-current heating bar;
Step 2: degassed: after foundry alloy fusing, vacuum outgas 15min ~ 20min;
Step 3: refining: be filled with high-purity argon gas to 0.1MPa in powder by atomization stove, by the foundry alloy liquation of melting at 1600 DEG C ~ 1650 DEG C temperature range inside holding 10min ~ 15min;
Step 4: atomization: the foundry alloy liquation of melting is flowed down through mozzle with the mass flowrate of 5kg/min ~ 10kg/min, with the high pressure of 3MPa ~ 5MPa, high-purity argon gas, metal liquid stream is broken into fine drop, drop is through supercooling and solidify formation spherical powder, enters and receives in powder tank;
Step 5: screening: powder is after fully cooling, and sieve under high-purity argon gas atmosphere, Sieving and casing less than 50 μm powder carry out Vacuum Package;
Described high-purity argon gas purity is 99.999wt%, and wherein oxygen content is less than 0.0001wt%.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104858440A (en) * | 2015-05-20 | 2015-08-26 | 武汉钢铁(集团)公司 | Method for preparing metal spherical powder for material increase manufacturing |
| CN105397085A (en) * | 2015-10-16 | 2016-03-16 | 中南大学 | Method for preparing nickel-based powder superalloy through spark plasma sintering |
| CN106216703A (en) * | 2016-09-27 | 2016-12-14 | 中航迈特粉冶科技（北京）有限公司 | A kind of preparation method of 3D printing spherical aluminum alloy powder |
| CN108097948A (en) * | 2017-12-22 | 2018-06-01 | 北京机科国创轻量化科学研究院有限公司 | A kind of anti-oxidation high-temperature heat treatment method of metal alloy attritive powder |
| CN108500279A (en) * | 2018-05-15 | 2018-09-07 | 南京尚吉增材制造研究院有限公司 | Cold hearth melting formula gas-atomised powders preparation method and device |
| CN108941588A (en) * | 2018-07-27 | 2018-12-07 | 中南大学 | A kind of preparation method of laser forming Ni-base Superalloy Powder |
| CN109338158A (en) * | 2018-12-24 | 2019-02-15 | 南通金源智能技术有限公司 | 3D printing titanium alloy powder and its atomization production |
| CN109759598A (en) * | 2019-03-20 | 2019-05-17 | 金川集团股份有限公司 | A kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder |
| CN109943752A (en) * | 2019-03-19 | 2019-06-28 | 江苏新华合金电器有限公司 | Plasma is atomized nickel base superalloy increasing material manufacturing wire rod and powder and preparation process |
| CN113084181A (en) * | 2021-04-12 | 2021-07-09 | 辽宁冠达新材料科技有限公司 | Preparation method of GH3230 nickel-based superalloy powder for 3D printing |
| CN113369484A (en) * | 2021-06-08 | 2021-09-10 | 金川镍钴研究设计院有限责任公司 | Method for preparing low-oxygen-content vacuum gas atomization 3D printing high-temperature alloy powder |
| CN113817935A (en) * | 2021-08-18 | 2021-12-21 | 盘星新型合金材料(常州)有限公司 | High-purity nickel-based high-temperature alloy and preparation method of spherical powder thereof |
| WO2022042088A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Nickel-based high-temperature alloy for 3d printing and preparation method for powder thereof |
| WO2022041252A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Method for eliminating cracks during 3d printing with nickel-based superalloy |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104858440A (en) * | 2015-05-20 | 2015-08-26 | 武汉钢铁(集团)公司 | Method for preparing metal spherical powder for material increase manufacturing |
| CN105397085A (en) * | 2015-10-16 | 2016-03-16 | 中南大学 | Method for preparing nickel-based powder superalloy through spark plasma sintering |
| CN106216703A (en) * | 2016-09-27 | 2016-12-14 | 中航迈特粉冶科技（北京）有限公司 | A kind of preparation method of 3D printing spherical aluminum alloy powder |
| CN108097948B (en) * | 2017-12-22 | 2019-11-05 | 北京机科国创轻量化科学研究院有限公司 | A kind of high-temperature heat treatment method that metal alloy attritive powder is anti-oxidation |
| CN108097948A (en) * | 2017-12-22 | 2018-06-01 | 北京机科国创轻量化科学研究院有限公司 | A kind of anti-oxidation high-temperature heat treatment method of metal alloy attritive powder |
| CN108500279A (en) * | 2018-05-15 | 2018-09-07 | 南京尚吉增材制造研究院有限公司 | Cold hearth melting formula gas-atomised powders preparation method and device |
| CN108941588A (en) * | 2018-07-27 | 2018-12-07 | 中南大学 | A kind of preparation method of laser forming Ni-base Superalloy Powder |
| CN108941588B (en) * | 2018-07-27 | 2020-04-10 | 中南大学 | Preparation method of nickel-based superalloy powder for laser forming |
| CN109338158A (en) * | 2018-12-24 | 2019-02-15 | 南通金源智能技术有限公司 | 3D printing titanium alloy powder and its atomization production |
| CN109943752A (en) * | 2019-03-19 | 2019-06-28 | 江苏新华合金电器有限公司 | Plasma is atomized nickel base superalloy increasing material manufacturing wire rod and powder and preparation process |
| CN109759598A (en) * | 2019-03-20 | 2019-05-17 | 金川集团股份有限公司 | A kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder |
| WO2022042088A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Nickel-based high-temperature alloy for 3d printing and preparation method for powder thereof |
| WO2022041252A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Method for eliminating cracks during 3d printing with nickel-based superalloy |
| US20220062992A1 (en) * | 2020-08-30 | 2022-03-03 | Central South University | Nickel-based superalloy for 3d printing and powder preparation method thereof |
| CN113084181A (en) * | 2021-04-12 | 2021-07-09 | 辽宁冠达新材料科技有限公司 | Preparation method of GH3230 nickel-based superalloy powder for 3D printing |
| CN113369484A (en) * | 2021-06-08 | 2021-09-10 | 金川镍钴研究设计院有限责任公司 | Method for preparing low-oxygen-content vacuum gas atomization 3D printing high-temperature alloy powder |
| CN113817935A (en) * | 2021-08-18 | 2021-12-21 | 盘星新型合金材料(常州)有限公司 | High-purity nickel-based high-temperature alloy and preparation method of spherical powder thereof |
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